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Catalyst for preparing trichloroethylene from 1,1,1,2-tetrafluoroethane

A technology of trifluoroethylene and tetrafluoroethane, used in physical/chemical process catalysts, dehydrohalogenation preparation, organic chemistry, etc., can solve the problems of low catalytic activity and fast deactivation of catalysts, and achieve high catalytic activity and catalyst Long life, short life effect

Active Publication Date: 2016-01-20
湖北孚诺林新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, the catalyst for preparing trifluoroethylene from HFC-134a has the problem of low catalytic activity, diluent gas needs to be introduced during the reaction process, and the catalyst deactivates quickly.

Method used

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  • Catalyst for preparing trichloroethylene from 1,1,1,2-tetrafluoroethane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Add 1 mol of alumina in a polytetrafluoroethylene reaction bottle, add water and stir to obtain a slurry, add 90 g of hydrofluoric acid with a mass concentration of 40% dropwise, filter, wash the filter cake until neutral, and dry it in an oven at 80 ° C. Calcined at 430°C for 4h in a muffle furnace to obtain Al 2 o 2.1 f 1.8 , the Al 2 o 2.1 f 1.8 Put into the flask, impregnate ferric nitrate, ferric nitrate and Al 2 o 2.1 f 1.8 The mass ratio is 0.01:1, dried in an oven at 80°C, and calcined in a muffle furnace at 430°C for 4h to make a catalyst 0.01Fe / Al 2 o 2.1 f 1.8 . Through evaluation, the conversion rate of HFC-134a is 63.2%, and the selectivity of trifluoroethylene reaches 98.9%.

Embodiment 2

[0017] Add 1 mol of alumina in a polytetrafluoroethylene reaction bottle, add water and stir to obtain a slurry, add 120 g of hydrofluoric acid with a mass concentration of 40% dropwise, filter, wash the filter cake until neutral, and dry it in an oven at 90 ° C. Calcined at 450°C for 3h in a muffle furnace to obtain Al 2 o 1.8 f 2.4 , the Al 2 o 1.8 f 2.4 Put into the flask, impregnate ferric nitrate, ferric nitrate and Al 2 o 1.8 f 2.4 The mass ratio of 0.05:1, dried in an oven at 90 ° C, roasted in a muffle furnace at 450 ° C for 3 hours, made into a catalyst, made into a catalyst 0.05Fe / Al 2 o 1.8 f 2.4 . Through evaluation, the conversion rate of HFC-134a is 67.4%, and the selectivity of trifluoroethylene reaches 99.2%.

Embodiment 3

[0019] Add 1 mol of alumina in a polytetrafluoroethylene reaction bottle, add water and stir to obtain a slurry, add 180 g of hydrofluoric acid with a mass concentration of 40% drop by drop, filter, wash the filter cake until neutral, and dry it in an oven at 100 ° C. Calcined at 470°C for 3h in a muffle furnace to obtain Al 2 o 1.2 f 3.6 , the Al 2 o 1.2 f 3.6 Put into the flask, impregnate ferric nitrate, ferric nitrate and Al 2 o 1.2 f 3.6 The mass ratio is 0.15:1, dried in an oven at 100°C, and roasted in a muffle furnace at 470°C for 3 hours to make a catalyst 0.15Fe / Al 2 o 1.2 f 3.6 . Through evaluation, the conversion rate of HFC-134a is 68.7%, and the selectivity of trifluoroethylene reaches 99.0%.

[0020] The catalyst of Example 3 was subjected to a life test, and the evaluation results are shown in Table 1.

[0021] Table 1 Life Test

[0022]

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Abstract

The invention discloses a catalyst for preparing trichloroethylene from 1,1,1,2-tetrafluoroethane. The catalyst has the composition of wM / Al2OxFy, wherein the Al2OxFy is an active carrier; 2x+y=6; the y is greater than or equal to 1.8, but smaller than or equal to 4.2; the M is an active ingredient and is selected from one of Fe, Zr, La or Ce; the w is the mass ratio of the M to the Al2OxFy; the w is greater than or equal to 0.01, but smaller than or equal to 0.2. The preparation method of the catalyst comprises the following steps that a liquid phase fluorination method is used for preparing the active carrier Al2OxFy; then, an equivalent impregnation method is used for loading one of ferric nitrate, zirconium nitrate, lanthanum nitrate or cerium nitrate to form the catalyst. The catalyst has the advantages that the activity is high; the conversion rate of 1,1,1,2-tetrafluoroethane during the reaction at 410 DEG C can reach more than 60 percent; the service life of the catalyst is long; the stable operation for 300h can be realized; in addition, the introduction of diluent gas is not needed in the reaction process; industrial application values are realized.

Description

technical field [0001] The invention relates to a catalyst, in particular to a catalyst for preparing trifluoroethylene from 1,1,1,2-tetrafluoroethane. Background technique [0002] Trifluoroethylene is not only an important polymer monomer, but also an important intermediate for the synthesis of many other compounds. Catalytic dehydrofluorination of 1,1,1,2-tetrafluoroethane (HFC-134a) to prepare trifluoroethylene is an economical and feasible route. The catalysts currently used to prepare trifluoroethylene from HFC-134a mainly include aluminum fluoride, MgF 2 -AlF 3 . [0003] U.S. Patent No. 5,856,593A reports that aluminum fluoride is used as a catalyst for preparing trifluoroethylene from HFC-134a. In the presence of diluent gas nitrogen, it reacts at 600 ° C. The initial conversion rate of HFC-134a can reach 34%, but the catalyst is quickly deactivated. After 190 min, the conversion of HFC-134a dropped to 5.8%. [0004] Wei Chen just reported the 5MgF 2 -AlF 3 a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/128B01J27/12B01J27/135C07C21/18C07C17/25
Inventor 白彦波吕剑毛伟王伟王博张伟秦越张振华
Owner 湖北孚诺林新材料有限公司
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